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1,2-Dichloroethane → HCID 59347881、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chloro-3-(trifluoromethyl)benzoic acid | HCID 2736677 | — |
| 反応物 | [2-Methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine | HCID 59347786 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 59347881 | HCID 59347881 | — |
反応手順
A mixture of [2-methyl-2-(2-methyl-1-pyrrolidinyl)-1-phenylpropyl]amine D26 (0.150 g; 0.647 mmol), 2-chloro-3-(trifluoromethyl)benzoic acid (0.174 g; 0.775 mmol), EDC (0.149 g; 0.777 mmol) and HOBt (0.020 g; 0.148 mmol) in DCM (4 ml) was shaken at room temperature for 66 hours. Saturated sodium hydrogen carbonate (8 ml) was added and shaking continued for 0.5 hours. The organic layer was passed through a phase separation cartridge and applied to a 2 g SCX column. The column was washed with DCM and methanol and the product eluted with 1M ammonia in methanol. The crude product was purified by chromatography on silica gel (20 g) eluting with 0-100% ethyl acetate in pentane gradient to afford the title compound as two pairs of enantiomers.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745642B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-d442d140b910474784016bfda8a268a9 |
| 出典メモ | uspto-grants-2010_06 |